HRID1907352

反应详情

EQUATION

反应方程式

HRID 1907352 反应方程式

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

8.78 g of ethyl [2-imino-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyridin-1-yl]acetate hydrobromide in 20 ml of POCl3 are placed in a round-bottomed flask. The reaction mixture is heated at 105° C. for 16 h, cooled to ambient temperature and concentrated under reduced pressure. The residue is taken up between dichloromethane and water at 0° C., and a 30% aqueous solution of NH4OH is added until a basic pH is obtained. The organic phase is separated, dried over magnesium sulphate and concentrated under reduced pressure. 4.3 g of compound are obtained.

WORKUP

后处理

  1. temperaturecooled to ambient temperature
  2. concentrationconcentrated under reduced pressure
  3. customis taken up between dichloromethane and water at 0° C.
  4. additiona 30% aqueous solution of NH4OH is added until a basic pH
  5. customis obtained
  6. customThe organic phase is separated
  7. dry with materialdried over magnesium sulphate
  8. concentrationconcentrated under reduced pressure